- Coupling of Bioreaction and Separation via Novel Thermosensitive Ionic Liquids Applied in the Baker’s Yeast-Catalyzed Reduction of Ethyl 2-oxo-4-phenylbutyrate
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The use of baker’s yeast to reduce ethyl 2-oxo-4-phenylbutyrate (EOPB) in conventional biphasic systems is hindered by low productivities due to mass transfer resistance between the biocatalyst and the substrate partitioned into two different phases. To overcome the limitation, a new reaction-separation coupling process (RSCP) was configured in this study, based on the novel thermosensitive ionic liquids (ILs) with polyoxyethylene-tail. The solubility of ILs in common solvents was investigated to configure the unique thermosensitive ionic liquids–solvent biphasic system (TIBS) in which the reduction was performed. [(CH3)2N(C2H5)(CH2CH2O)2H][PF6] (c2) in 1,2-dimethoxyethane possesses the thermosensitive function of homogeneous at lower temperatures and phase separating at higher temperatures. The phase transformation temperature (PTT) of the mixed system of c2/1,2-dimethoxyethane (v/v, 5:18) was about 33 ?C. The bioreaction takes place in a “homogeneous” liquid phase at 30 ?C. At the end of each reduction run, the system temperature is increased upon to the PTT, while c2 is separated from 1,2-dimethoxyethane with turning the system into two phases. The enantiomeric excesses (e.e.) of ethyl (R)-2-hydroxy-4-phenylbutyrate ((R)-EHPB) increased about 25~30% and the yield of ethyl-2-hydroxy-4-phenylbutyrate (EHPB) increased 35% in TIBS, compared with the reduction in 1,2-dimethoxyethane. It is expected that the TIBS established in this study could provide many future opportunities in the biocatalysis.
- Feng, Lifang,Shi, Yugang,Tian, Shiyi,Yang, Yuexi
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- Method for homogeneously catalyzing alcohol amination
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The invention relates to a method for homogeneously catalyzing alcohol amination. The method comprises the following steps: mixing diethylene glycol or 1,6-hexanediol, dimethylamine, a ruthenium metalcatalyst and a non-polar solvent and carrying out homogeneous catalysis reaction; separating. According to the method provided by the invention, under the catalysis of a noble metal (rhodium, ruthenium and iridium) metallic catalyst, the diethylene glycol which has a cheap price and is easy to obtain or the 1,6-hexanediol is directly subjected to the amination by utilizing the dimethylamine through a one-step method; bis(2-dialkylaminoethyl)ether or N,N,N,N-tetramethylhexanediamine is prepared in a high-conversion-rate and high-selectivity manner.
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Paragraph 0068-0074
(2019/02/21)
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- Integrated preparation method of DMAE and DMAEE in microtubule reactor
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The invention discloses an integrated preparation method of DMAE and DMAEE in a microtubule reactor. The method comprises respectively feeding ethylene oxide and an aqueous solution of dimethylamine and water as a catalyst into a micro-tube reactor through a pump according to a mole ratio of ethylene oxide to dimethylamine oo 1-2: 1, setting a reaction temperature in the micro-tube reactor to 60-90 DEG C and pressure to 1.3+/-0.2 Pa and controlling standing time of the materials in the micro-tube reactor in 15-90s, wherein the efflux from the micro-tube reactor is an aqueous solution of DMAE and DMAEE. The method has the advantages of high atomic economy, good reaction selectivity, mild reaction conditions, short reaction time, simple catalyst and simple product separation.
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Paragraph 0035-0036; 0042
(2018/03/23)
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- Bis(2-dimethylaminoethyl)ether synthesis method
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The invention belongs to the technical field of organic macromolecular compounds and relates to a bis(2-dimethylaminoethyl)ether synthesis method. The method includes subjecting dimethylamine and ethylene oxide to reaction in a high-pressure reactor, wherein a mole ratio is 1:2-2.2, a reaction temperature is 60-100 DEG C, reaction time is 2-5 hours, and curing time is 0.5-1 hour; adding a catalyst Cu-Ni/gamma-Al2O3, adopting hydrogen for adjusting an internal pressure of the reactor to 1.5-2.5 MPa, controlling the temperature at 190-220 DEG C, controlling a reaction pressure to be 10-25 MPa, and reacting for 6-13h; after the pressure drops to 1.0 MPa, feeding to the middle of an amine/hydrogen removal tower to discharge the dimethylamine and the hydrogen in the mixture from the top of the amine/hydrogen removal tower, and subjecting a crude product of bis(2-dimethylaminoethyl)ether at the bottom of the amine/hydrogen removal tower to reduced pressure distillation and separation. The bis(2-dimethylaminoethyl)ether synthesis method is applied to polyether preparation and has advantages of high equipment utilization rate, high preparation efficiency and the like.
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Paragraph 0038; 0039; 0040; 0041; 0050; 0056; 0059; 0062
(2017/06/10)
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- Synthesizing method of N, N-dimethyl diglycolamine
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The invention discloses a synthesizing method of N, N-dimethyl diglycolamine. The method comprises the following steps: adding diglycolamine and paraformaldehyde to a vessel, and dropwise adding formic acid in stirring, wherein the molar ratio of diglycolamine to paraformaldehyde to formic acid is 1: (2-3): (2-3), and the reaction is carried out for 1-2 hours at the temperature of 50 to 110 DEG C; performing pressure-reduction steaming to obtain water generated in the reaction after the reaction is finished, so as to obtain the reacting liquid; adding alcohols substances to the obtained reacting liquid to perform an ester exchange reaction so as to obtain the purified reacting liquid; and performing pressure-reduction distilling on the obtained purified reacting liquid so as to separate out the alcohols substances and N, N-dimethyl diglycolamine, wherein the alcohols substances can be recycled.
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Paragraph 0043-0058; 0064
(2017/07/19)
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- NOVEL NITRILE AND AMIDOXIME COMPOUNDS AND METHODS OF PREPARATION
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The present application relates to semiconductor processing compositions comprising at least one compound containing at least one amidoxime functional group and to methods of using these compositions in semiconductor processing. The present application also describes the preparation of amidoximes for a semiconductor processing composition by (a) mixing a cyanoethylation catalyst, a nucleophile and an alpha-unsaturated nitrile to produce a cyanoethylation product; and (b) converting a cyano group in the cyanoethylation product into an amidoxime functional group.
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- METHOD FOR THE CONTINUOUS PRODUCTION OF AN AMINE
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The invention relates to a method for the continuous production of an amine by reacting a primary or secondary alcohol, aldehyde and/or ketone with hydrogen and a nitrogen compound, selected from the group containing ammonia and primary and secondary amines, at a temperature that ranges between 60 and 300 °C in the presence of a catalyst containing copper. According to the invention, the catalytically active mass of the catalyst contains the following prior to its reduction with hydrogen: 20 to 85 wt. % aluminium oxide (Al2O3), zirconium dioxide (ZrO2), titanium dioxide (TiO2) and/or silicon dioxide (SiO2); 1 to 70 wt. % copper compounds containing oxygen, calculated as CuO; 0 to 50 wt. % magnesium compounds containing oxygen, calculated as MgO; chromium compounds containing oxygen, calculated as Cr2O3; zinc compounds containing oxygen, calculated as ZnO; barium compounds containing oxygen, calculated as BaO; and/or calcium compounds containing oxygen, calculated as CaO; and less than 30 wt. % nickel compounds containing oxygen, calculated as NiO, in relation to the copper compounds containing oxygen, calculated as CuO. The reaction in the gas phase takes place isothermally in a tubular reactor.
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Page/Page column 25
(2008/06/13)
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- Enhanced product selectivity in continuous N-methylation of amino alcohols over solid acid-base catalysts with supercritical methanol
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The unique properties of supercritical fluids can be exploited for fine-tuning product selectivity. Under the conditions listed for the N-methylation of amino alcohols (see scheme) over solid acid-base bifunctional catalysts, the total yield and product selectivity could be improved. Enhanced product selectivity might be attributed to the milder reaction conditions possible with supercritical methanol, as well as the increased concentration of methanol on the catalyst.
- Oku, Tomoharu,Ikariya, Takao
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p. 3476 - 3479
(2007/10/03)
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- 1,2-Di-O-hexadecylglycero-3-phosphocholines with ethylene glycol units adjacent to the head group
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We synthezised a number of racemic 1,2-Di-O-hexadecylglycero-3-phosphocholines with hydrophilic ethylenglycol units (EO)(n) (with n = 1-3) adjacent to the choline of the head group and studied their lyotropic phase behaviour in excess water (50 weight%) by differential scanning calorimetry (DSC). The behaviour of the compounds was compared with that of the unsubstituted rac-1,2-Di-O-hexadecylglycero-3-phosphocholin (DHPC). Our results indicate that there is almost no difference in the phase behaviour and in the water adsorption after introduction of one EO-unit. In contrast to this, the compounds with two and three EO-units show a changed polymorphic behaviour with increased temperature, enthalpy and entropy of the main transition and a higher adsorption of water.
- Rattay,Rettig
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p. 676 - 679
(2007/10/03)
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